CN109680257A - A kind of preparation method of nano material - Google Patents
A kind of preparation method of nano material Download PDFInfo
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- CN109680257A CN109680257A CN201910123904.6A CN201910123904A CN109680257A CN 109680257 A CN109680257 A CN 109680257A CN 201910123904 A CN201910123904 A CN 201910123904A CN 109680257 A CN109680257 A CN 109680257A
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- C23C16/02—Pretreatment of the material to be coated
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/02—Pretreatment of the material to be coated
- C23C14/028—Physical treatment to alter the texture of the substrate surface, e.g. grinding, polishing
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
- C23C14/0605—Carbon
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/02—Pretreatment of the material to be coated
- C23C16/0254—Physical treatment to alter the texture of the surface, e.g. scratching or polishing
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C16/00—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes
- C23C16/22—Chemical coating by decomposition of gaseous compounds, without leaving reaction products of surface material in the coating, i.e. chemical vapour deposition [CVD] processes characterised by the deposition of inorganic material, other than metallic material
- C23C16/26—Deposition of carbon only
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Abstract
The invention discloses a kind of preparation methods of nano material, using a kind of material as base material, uniformly or non-uniformly microcosmic pit structure is formed in the substrate material surface, carbon nanotube is grown in the substrate material surface again, the root for the carbon nanotube being in contact with substrate is embedded in the pit-hole of substrate material surface.Microcosmic cratered hole structural substrates are used in the present invention, the root of the carbon nanotube grown can be embedded in the pit-hole of substrate material surface, it is easy Automatic-falling with the carbon nanotube grown on smooth substrate material surface or is compared the case where scraping, carbon nanotube root in the technology of the present invention is securely fixed by porous pit structure, to make carbon nanotube be not easy to fall off from substrate material surface or be scraped, the binding force between carbon nanotube and base material is greatly improved.
Description
Technical field
The invention belongs to field of nanometer material technology, in particular to a kind of preparation method of nano material, to improve carbon nanotube
Binding force between substrate.
Background technique
Carbon nano-tube material has had been a concern research since being found, as a kind of typical one-dimensional material, carbon
Nanotube has excellent performance in chemistry, physics, electronics and mechanical aspects, as carbon nanotube have it is excellent conductive, thermally conductive
Performance, high mechanical strength, stronger wideband electromagnetic wave-absorbing property etc., make carbon nanotube in physics, chemistry and material supply section
It is widely studied and is applied in etc. fields.Currently, carbon nanotube, which is widely used, makees electrode material for super capacitor, enhancing
Material, gas adsorption material, catalysis material, field electron emission materials, heat conducting material and sensing material etc..
It is individually sharp but in as many application practices such as electrode material, thermal conducting material, reinforcing material, electronic material
It uses carbon nanotube to be not easy to realize as independent electrode, heat transfer, reinforcing material or electronic material, needs to utilize a kind of base
The collector of the performances such as electric current, heat transfer of the bottom material as the carbon nanotube grown, to give full play to and utilize carbon nanometer
The performances such as excellent conductive, the thermally conductive, electromagnetic shielding of pipe.Metal and its alloy material or metal oxide materials etc., all may be used
As the base material of carbon nano tube growth, can be applied to not with the carbon nano-tube material prepared together as composite material
Same technical field.
Laser evaporization method, graphite acr method, pyrolyzed-polymer method etc. can be used in the preparation method of carbon nanotube, grinds in experiment
Study carefully and also often grows carbon nanotube in different substrate material surfaces using chemical vapour deposition technique in production practices.But not Tongfang
The not strong problem of generally existing binding force between the carbon nanotube and substrate that method is prepared, in substrate and carbon nano tube compound material
Practical application during easily there is carbon nanotube and fall off from substrate, cause that the performance of the device of preparation is unstable, service life contracting
The problems such as short.Therefore, improving binding force between carbon nanotube and substrate is the critical issue in composite material application process.For
This critical issue, lot of domestic and international researcher improve the binding force between carbon nanotube and base material by distinct methods.
Such as: Shaijumon et al. improved using golden boundary material aligned carbon nanotube as electrode material for super capacitor and
Binding force between copper-based bottom；M.Dharmendra et al. is improved using diamond transition zone between carbon nanotube and copper-based bottom
Binding force and heat-conductive characteristic；Lin Wei et al. copper substrate surfaces using Atomic layer deposition method deposit one layer of pellumina come
It grows carbon nanotube and improves binding force Huan-Chieh Su et al. between carbon nanotube and copper-based bottom and utilize microwave handling method
Carbon nanotube is embedded to the binding force improved between carbon nanotube and titanium substrate in titanium substrate；Seong Chu Lim utilizes heat sink
Product method deposits indium and tin metal layer on indium-tin oxide glass surface to enhance carbon nanotube and substrate caking power；Zhu Lingbo
Et al. propose to improve binding force between carbon nanotube and substrate by reflow soldering method.Hironori Kumagai et al.
(US2009/0317597Al) one layer of porous coating is prepared using in substrate surface, the carbon that orientation is grown on porous coating is received
After mitron, the porous coating of nano thickness is subjected to high temperature melting, so that carbon nanotube is fixed on substrate surface.But
The step of all of above method is all multistage method, and carbon nanotube and substrate caking power are improved in many technical methods is very multiple
Miscellaneous, cost also can be very high.Therefore, it finds a kind of simple, at low cost and is conducive to the raising carbon nanometer applied in large-scale production
The technical method of binding force is highly desirable between pipe and base material.
Summary of the invention
The present invention be exactly in order to solve during above-mentioned raising carbon nanotube and substrate caking power and
One kind of offer is simple, application of easily accomplishing scale production, cost is relatively low and be greatly improved carbon nanotube and base material it
Between binding force technological invention.
For the not strong technical problem of the carbon nanotube and substrate caking power of solution chemical vapour deposition technique growth, the present invention is
It is implemented with the following technical solutions.
A kind of preparation method of nano material, which is characterized in that using a kind of material as base material, in the substrate material
Expect that surface forms uniformly or non-uniformly microcosmic pit structure, then raw in the substrate material surface with microcosmic pit structure
The root of long carbon nanotube, the carbon nanotube being in contact with substrate is embedded in the pit-hole of substrate material surface, the pit-hole surface
Shape is round, oval, rectangular, triangle or irregular shape, in pit-hole shape be ball-shaped, cubic type, cylindrical type,
Pyramid type or irregular three-dimensional shape are interconnected between pit-hole or are not connected to mutually.
Further, the pit-hole and substrate surface vertical depth are 2 μm~50 μm.
Further, the pit-hole surface apertures are less than internal aperture, and pit-hole surface apertures length is 0.1 μm~50 μm.
Further, pit-hole by chemistry, electrochemical etching method or physics polish-brush, rolling, sandblasting, shot-peening, laser ablation,
Method for etching plasma is formed.
Further, base material is metallic iron and ferrous alloy, metallic nickel and nickel-base alloy, Titanium and titanium-base alloy
With titanium dioxide, metallic copper and acid bronze alloy, metallic aluminium and acieral or aluminium oxide, silicon and silica, quartz, metal platinum
And platinum base alloy, gold and its alloy, metallic silver and its alloy, glass material.
Further, using the methods of laser evaporization method, graphite acr method, chemical vapour deposition technique in the base material
Surface grows carbon nanotube, and substrate material surface is first specially pre-processed simultaneously supported catalyst or to substrate surface without pre-
After handling simultaneously supported catalyst, base material is put into carbon nano tube growth reaction unit, it is different according to selected selection method, lead to
Enter protective gas, reducing gas, carbon-source gas, catalyst, in 400 DEG C of -1000 DEG C of temperature ranges, described with special
The substrate surface of porous structure grows carbon nano-tube material.
Advantageous effects of the invention:
Cratered hole substrate is used in the present invention, the root of the carbon nanotube grown can be embedded to the pit-hole of substrate material surface
In, it is easy Automatic-falling with the carbon nanotube grown on smooth substrate material surface or is compared the case where scraping, the present invention
Carbon nanotube root in technology is securely fixed by porous pit structure, so that carbon nanotube be made to be not easy from base material table
Emaciated face falls or is scraped, and greatly improves the binding force between carbon nanotube and base material.
Detailed description of the invention
Fig. 1 is the upper surface scanning electron microscope (SEM) photograph for the cratered aluminum foil substrate of tool selected in the technical program embodiment；
Fig. 2 is the cross-sectional scans electron microscope for the cratered aluminum foil substrate of tool selected in the technical program embodiment；
Fig. 3 be in the technical program embodiment have carbon nanotube prepared by cratered aluminum foil substrate material surface with
And carbon nanotube and substrate are in contact the stereoscan photograph at interface.
Fig. 4 is the peel strength of respectively the technical program embodiment 1 and the carbon nanotube of smooth aluminium foil surface preparation
Test result comparison diagram.
Specific embodiment
The following describes the present invention in detail with reference to the accompanying drawings and specific embodiments.
The not strong technical problem of the carbon nanotube and substrate caking power grown in relative smooth substrate for solution, the present invention
Adopt the following technical solutions realization.
1. selecting a kind of for growing the base material of carbon nanotube, this base material can be metallic iron and iron-based conjunction
Gold, metallic nickel and nickel-base alloy, Titanium and titanium-base alloy and titanium dioxide, metallic copper and acid bronze alloy, metallic aluminium and aluminium base
Alloy or aluminium oxide, silicon and silica, metal platinum and platinum base alloy, gold and its alloy, metallic silver and its alloy, glass material
Material.
2. this substrate material surface can utilize chemistry, electrochemical etching method or physics polish-brush, rolling, sandblasting, shot-peening, swash
Lithographic methods form uniformly or non-uniformly microcosmic pit structure, and pit-hole and substrate surface vertical depth are 2 μm~50 μm, often
A pit-hole mouth can be round, oval, rectangular, triangle or irregular shape, and pit-hole aperture length is 0.1 μm~50 μm,
Shape can be ball-shaped, cubic type, cylindrical type, pyramid type or irregular three-dimensional shape in pit-hole, can phase between pit-hole
It is intercommunicated or be not connected to mutually；
3. carbon nanotube can be specifically described as two classpaths in the process of the substrate surface growth with microcosmic pit structure:
(1) will there is the substrate material surface of microcosmic pit structure to form one layer to be used to grow carbon nanotube by pretreatment
Catalyst film layer, then base material is put into reaction unit, is passed through protective gas, carbon-source gas, reducing gas, delivery
Gas grows carbon nanotube in the substrate surface with microcosmic pit structure at 400 DEG C -1000 DEG C；
(2) substrate material surface with microcosmic pit structure does not pre-process supported catalyst, and base material is put into instead
It answers in furnace, be passed through protective gas, carbon-source gas, catalyst, reducing gas, delivery gas has at 400 DEG C -1000 DEG C
The substrate surface of microcosmic pit structure grows carbon nanotube.
4. the carbon nanotube grown on the base material that surface has microcosmic pit-hole pit-hole, the carbon being in contact with substrate
The root of nanotube can be embedded in the pit-hole of substrate material surface, so that it is de- from substrate material surface to guarantee that carbon nanotube is not easy
It falls, greatly improves the binding force between carbon nanotube and base material, in addition, if control pit-hole surface apertures are less than internal holes
Diameter can then further increase the binding force between carbon nanotube and base material on this basis.The so-called aperture of the present invention is
The distance of the farthest point-to-point transmission of distance on the same plane of finger-hole.
Embodiment 1
Corrode the pit-hole that vertical depth out is about 2 μm -10 μm or so in aluminum foil substrate material surface using electrochemical method,
Shape is irregular three-dimensional cavity in pit-hole, and base material is put into chemical gas by 0.1 μm -10 μm of pit-hole surface bore length
In phase deposition reaction furnace, it is passed through argon gas as protective gas, base material is warming up to 625 DEG C, heat preservation, and to chemical vapor deposition
It is passed through hydrogen, the ethanol solution dissolved with catalyst ferrocene, ethylene gas in product reacting furnace, is started raw on aluminum foil substrate surface
The root of long carbon nanotube, reaction time 1h, the interface that the carbon nanotube prepared is contacted with aluminum foil substrate, carbon nanotube twines
It is coiled into similar small Coiling-type, is embedded in the pit-hole on aluminum foil substrate surface, to greatly improve the knot of carbon nanotube and aluminum foil substrate
With joint efforts.
Embodiment 2
Use the method for laser ablation silicon oxide ceramics surface etch go out vertical depth for 30 μm -50 μm circle it is recessed
Hole, pit are the circular cavity that inside diameter is greater than pit surface bore, and pit surface bore length is 15 μm, with pit
The Fe catalyst layer of one layer of about 30nm thickness is deposited in the silica material surface on surface, and load is then had catalyst film layer
Oxidation silicon base is put into chemical vapour deposition reactor furnace, is passed through argon gas as protective gas, base material is warming up to 950
DEG C, heat preservation, and hydrogen, ethylene gas are passed through into chemical vapour deposition reactor furnace, start to grow carbon in oxidation silicon substrate surface
Nanotube, reaction time 1h, the interface that the carbon nanotube prepared is contacted with oxidation silicon base, the root winding of carbon nanotube
It at similar small Coiling-type, is embedded in the pit-hole of substrate material surface, to greatly improve carbon nanotube and aoxidize the knot of silicon base
With joint efforts.
Embodiment 3
Corroding vertical depth out in the Ni-based stainless steel substrate material surface of iron using chemical method is about 2 μm -20 μm or so
Pit-hole, shape is irregular three-dimensional cavity in pit-hole, and base material is put by 0.1 μm -20 μm of pit-hole surface bore length
In chemical vapour deposition reactor furnace, it is passed through argon gas as protective gas, base material is warming up to 800 DEG C, heat preservation, and to chemistry
It is passed through hydrogen, the ethanol solution dissolved with ferrum-based catalyst, acetylene gas in vapor deposition reaction furnace, starts in stainless steel base
Surface growth carbon nanotube, reaction time 1h, the interface that the carbon nanotube prepared is contacted with iron nickel and stainless steel substrate, carbon are received
The root of mitron is wound in similar small Coiling-type, is embedded in the pit-hole of stainless steel substrate surface, to greatly improve carbon nanotube
With the binding force of stainless steel base.
Embodiment 4
Going out vertical depth in titanium substrate material etch using the method for plasma etching is about 5 μm or so uniform
The ellipse pit-hole of distribution, shape is oval three-dimensional cavity, 2 μm -5 μm of pit-hole surface bore length, by base material in pit-hole
It is put into chemical vapour deposition reactor furnace, is passed through argon gas as protective gas, base material is warming up to 700 DEG C, is kept the temperature, and to
It is passed through hydrogen, catalyst, ethylene gas in chemical vapour deposition reactor furnace, starts to grow carbon nanometer on titanium substrate surface
Pipe, the root of reaction time 1h, the interface that the carbon nanotube prepared is contacted with titanium substrate, carbon nanotube are wound in class
Like small Coiling-type, it is embedded in the pit-hole on titanium substrate surface, to greatly improve the combination of carbon nanotube and titanium substrate
Power.
Embodiment 5
Go out the pit-hole that vertical depth is about 25 μm or so, pit-hole table in glass material surface corrosion using chemical corrosion method
Face bore is about 5 μm -50 μm, and shape is nearly rectangle solid cavity in pit-hole, and base material is put into plasma enhancing
It learns in vapor deposition reaction furnace, is passed through argon gas as protective gas, base material is warming up to 450 DEG C, is kept the temperature, and to chemical gas
It is passed through hydrogen, catalyst, ethylene gas in phase deposition reaction furnace, starts to grow carbon nanotube on glass substrate material surface, instead
1h between seasonable, the interface that the carbon nanotube prepared is contacted with substrate of glass, the root of carbon nanotube are wound in similar small line
Bulk is embedded in the pit-hole of glass basic surface, to greatly improve the binding force of carbon nanotube and substrate of glass.
Embodiment 6
The pit-hole that vertical depth is about 10 μm or so, pit-hole table are etched in copper substrate surfaces using rolling, polish-brush method
Face bore is about 30 μm -50 μm, and shape is polyhedral solid cavity in pit-hole, and substrate material surface is coated a layer thickness about
After 30nm aluminum oxide film layer, copper-based bottom is put into chemical vapour deposition reactor furnace, is passed through argon gas as protective gas, by substrate
Material warms are to 750 DEG C, heat preservation, and hydrogen, catalyst, ethylene gas are passed through into chemical vapour deposition reactor furnace, start
Copper base material surface grows carbon nanotube, reaction time 1h, the interface that the carbon nanotube prepared is contacted with copper-based bottom, carbon
The root of nanotube is wound in similar small Coiling-type, is embedded in the pit-hole of copper substrate surfaces, thus greatly improve carbon nanotube and
The binding force at copper-based bottom.
Comparative example
Fig. 4 is in the technical program embodiment 1 in the cratered aluminum foil substrate material surface of tool and in smooth aluminium foil table
After wheat flour is for carbon nanotube, the comparison diagram of 180 ° of peel strength test results is carried out with reference to GB2792-1998.As shown,
It is higher than in the peel strength of the carbon nanotube of the substrate surface growth with microcosmic pit structure and is grown on smooth substrate surface
Carbon nanotube peel strength.In addition, after peel strength test, on smooth substrate surface, the carbon nanotube of growth has been
It is detached from from aluminum foil substrate completely, and is still firmly fixed to aluminium foil table in the carbon nanotube for having cratered substrate surface growth
Face (as shown in illustration in Fig. 4).
Above-described is only presently preferred embodiments of the present invention, not limitation invention.It should be understood that for the general of this field
For logical technical staff, under technical inspiration provided by the present invention, other equivalent improvement can also be made, this may be implemented
The purpose of invention, is regarded as protection scope of the present invention.
Claims (5)
1. a kind of preparation method of nano material, which is characterized in that using a kind of material as base material, in the base material
Surface forms uniformly or non-uniformly microcosmic pit structure, then in the substrate material surface growth with microcosmic pit structure
The root of carbon nanotube, the carbon nanotube being in contact with substrate is embedded in the pit-hole of substrate material surface, pit-hole surface shape
Shape is round, oval, rectangular, triangle or irregular shape, and shape is ball-shaped, cubic type, cylindrical type, circle in pit-hole
Tapered or irregular three-dimensional shape is interconnected between pit-hole or is not connected to mutually.
2. the preparation method of nano material according to claim 1, which is characterized in that the pit-hole is vertical with substrate surface
Depth is 2 μm~50 μm.
3. the preparation method of nano material according to claim 1 or 2, which is characterized in that the pit-hole surface apertures are small
In internal aperture, pit-hole surface apertures length is 0.1 μm~50 μm.
4. the preparation method of nano material according to claim 3, which is characterized in that pit-hole is by chemistry, electrochemical corrosion
Method or physics polish-brush, rolling, sandblasting, shot-peening, laser ablation, method for etching plasma are formed.
5. the preparation method of nano material according to claim 3, which is characterized in that base material is metallic iron and iron-based
Alloy, metallic nickel and nickel-base alloy, Titanium and titanium-base alloy and titanium dioxide, metallic copper and acid bronze alloy, metallic aluminium and aluminium
Based alloy or aluminium oxide, silicon and silica, quartz, metal platinum and platinum base alloy, gold and its alloy, metallic silver and its alloy,
Glass material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112121328A (en) * | 2020-08-28 | 2020-12-25 | 重庆工程职业技术学院 | Fire control unit based on unmanned aerial vehicle |
| CN112844349A (en) * | 2019-11-28 | 2021-05-28 | 桂林理工大学 | Method for preparing TiOx photoanode by laser etching of Ti sheet |
| CN114989790A (en) * | 2022-04-26 | 2022-09-02 | 海南大学 | Method for synergistically optimizing TiO2 by using nickel/carbon nanotube and carbon layer, obtained product and application |
| CN115676806A (en) * | 2022-08-24 | 2023-02-03 | 西安交通大学 | Double-sided growth high-area-density vertical array carbon nanotube and preparation method and application thereof |
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